【摘要】 目的建立HPLC-MS/MS分析方法测定人血浆中的金刚烷胺浓度,并用于研究健康受试者口服氨酚咖黄烷胺片后金刚烷胺的药动学。方法血浆经乙醚-二氯甲烷(4∶1,V/V)提取,采用C18柱为分析柱,甲醇-10 mmol.L-1醋酸铵溶液-冰醋酸(60∶40∶0.08,V/V/V)为流动相,流速1.0 mL.min-1,柱后分流,0.2 mL.min-1进入质谱,柱温35℃。质谱检测方式:多反应离子监测,选择监测的离子为m/z152→m/z135(金刚烷胺)和m/z275→m/z230(内标物,氯苯那敏)。结果金刚烷胺的线性范围为1~200μg.L-1(r=0.9999),血浆中金刚烷胺的最低定量限达1μg.L-1(RS,N>10),回收率>80%。结论本法简便、准确、灵敏度高,适用于金刚烷胺的药动学研究。更多还原

【Abstract】 AIM To develop an LC-MS/MS assay to determine amantadine in human plasma and investigate the pharmacokinetics of amantadine after oral administration of the compound preparation.METHODS The plasma samples were extracted with ethyl ether-dichlormethane(4∶1,V/V).The separation was carried out on a Shimadzu ODS column(150 mm×4.6 mm,5μm) at 35℃.The mobile phase consisted of methanol,10 mmol·L-1 ammonium acetate and acetic acid(60∶40∶0.08,V/V/V),running at a flow rate of 1.0 mL·min-1.After separation,the mobile phase was splitted and 0.2 mL·min-1 was into MS.LC-MS/MS was performed in the MRM mode using target ions at m/z 152→m/z 135 for amantadine and m/z 275→m/z 230 for chlorphenamine.RESULTS The linear calibration curve was obtained in the concentration range of 1-200 μg·L-1(r=0.999 9).The lowest limit of quantification of amantadine in plasma was 1 μg·L-1.The average recovery was more than 80%.CONCLUSION The assay is proved to be sensitive,accurate and convenient.The method can be used for the pharmacokinetic research of amantadine.更多还原